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1 Electronic Supplementary Material (ESI) for Nanoscale. This journal is The Royal Society of Chemistry 2015 Supporting Information Synthesis and electrochemical properties of spherical and hollow-structured NiO aggregates created by combining the Kirkendall effect and Ostwald ripening Jung Sang Cho, Jong Min Won, Jong-Heun Lee, and Yun Chan Kang* Department of Materials Science and Engineering Korea University Anam-Dong, Seongbuk-Gu Seoul , Republic of Korea Keywords: Kirkendall diffusion; Ostwald ripening; nanopowders; nickel oxide; lithium ion battery; spray pyrolysis

2 Fig. S1 (a) XRD pattern, (b) TG curve, and (c) SEM image of the as-prepared precursor powders directly obtained by spray pyrolysis process.

3 Fig. S2. XRD patterns of the Ni-C composite powders obtained by reduction process at 300 o C under 10% H 2 /Ar gas and hollow NiO aggregates obtained by oxidation of the reduced Ni-C composite powders at 300 o C under air.

4 Fig. S3. Ni2p XPS spectra of the (a) Ni-C composite powders obtained by reduction process at 300 o C under 10% H 2 /Ar gas and (b) hollow NiO aggregates obtained by oxidation of the reduced Ni-C composite powders at 300 o C under air.

5 Fig. S4. TG curves of the (a) Ni-C composite powders obtained by reduction process at 300 o C under 10% H 2 /Ar gas and (b) hollow NiO aggregates obtained by oxidation of the reduced Ni-C composite powders at 300 o C under air.

6 Fig. S5 Morphologies, SAED pattern, XRD pattern, and elemental mapping images of the solid NiO aggregates obtained by direct oxidation of as-prepared precursor powders at 300 o C under air: (a) SEM, (b, c) TEM images, (d) HR-TEM image, (e) SAED pattern, (f) XRD pattern, and (g) elemental mapping images.

7 Fig. S6 Morphologies, SAED pattern, XRD pattern, and elemental mapping images of the hollow NiO shell obtained by spray pyrolysis: (a) SEM, (b, c) TEM images, (d) HR- TEM image, (e) SAED pattern, (f) XRD pattern, and (g) elemental mapping images.

8 Fig. S7. N 2 adsorption-desorption isotherms measured at 77 K for the hollow NiO aggregates, which were formed through the synergetic effects of nanoscale Kirkendall diffusion and Ostwald ripening, and solid NiO aggregates and hollow NiO shell.

9 Fig. S8. Pore size distributions of (a) hollow NiO aggregates, (b) solid NiO aggregates and (c) hollow NiO shell.

10 Fig. S9. Cyclic voltammogram (CV) curves of the (a) hollow NiO shell and (b) solid NiO aggregates for the first 5 cycles at a constant current density of 1.0 A g -1.

11 Fig. S10. Nyquist impedance plots of the (a) three samples before cycling and (b) solid NiO aggregates after cycling.

12 Fig. S11. Rate performances of the hollow NiO aggregates, which were formed through the synergetic effects of nanoscale Kirkendall diffusion and Ostwald ripening, and solid NiO aggregates and hollow NiO shell.

13 Fig. S12. TG curves of the (a) hollow NiO shell and (b) solid NiO aggregates.

14 Fig. S13. Hysteresis curves of the hollow NiO aggregates and solid NiO aggregates.

15 Table S1. Comparison of the electrochemical performances of the hollow NiO aggregates formed through the synergetic effect of nanoscale Kirkendall diffusion and Ostwald ripening with the reported results of the nanostructured nickel oxide materials. Materials Voltage range (V) Current rate Initial C dis /C cha [ma h g -1 ] Discharge capacity [ma h g -1 ] Cycle number Ref. spherical and hollow-structured NiO aggregates ma g / In this work NiO nanofibers ma g -1 ~1280/~784 ~ S1 NiO microspheres ma g /~ S2 NiO nanowall ma g /833 ~ S3 NiO nanoshafts ma g /~ S4 NiO/RuO 2 composite carbon nanofibers ma g -1 ~650/~ S5 NiO/MWCNT ma g / S6 2 core-shell nanopowders ma g / S7 porous NiO fiber ma g -1 ~1100/696 ~ S8 NiO hollow microspheres ma g / S9 NiO/grapheme ma g -1 ~1100/~ S10 NiO-C nanocomposite ma g / S11 NiO yolk-shell powders ma g -1 ~1200/ S12 NiO nanoflake arrays ma g /~ S13 Co-doped NiO nanoflake ma g / S14 Co-doped NiO nanoparticles ma g / S15 3D flower-like NiO ma g / S16 bamboo-like amorphous carbon nanotubes clad in ultrathin NiO nanosheets ma g / S17 References S1 V. Aravindan, P. Suresh Kumar, J. Sundaramurthy, W. C. Ling, S. Ramakrishna,

16 S. Madhavi, J. Power Sources, 2013, 227, S2 L. Liu, Y. Li, S. Yuan, M. Ge, M. Ren, C. Sun, Z. Zhou, J. Phys. Chem. C, 2010, 114, S3 B. Varghese, M. V. Reddy, Z. Yanwu, C. S. Lit, T. C. Hoong, G. V. S. Rao, B. V. R. Chowdari, A. T. S. Wee, C. T. Lim, C. H. Sow, Chem. Mater., 2008, 20, S4 L. Yuan, Z. P. Guo, K. Konstantinov, P. Munroe, H. K. Liu, Electrochem. Solid- State Lett. 2006, 9, A524-A528. S5 Y. Wu, R. Balakrishna, M. V. Reddy, A. S. Naira, B. V. R. Chowdari, S. Ramakrishna, J. Alloys Compd., 2012, 517, S6 C. Xu, J. Sun, L. Gao, J. Power Sources, 2011, 196, S7 S. H. Choi, J. H. Lee, Y. C. Kang, Nanoscale, 2013, 5, S8 B. Wang, J. L. Cheng, Y. P. Wu, D. Wang, D. N. He, Electrochem. Commun., 2012, 23, 5-8. S9 D. Xie, W. Yuan, Z. Dong, Q. Su, J. Zhang, G. Du, Electrochim. Acta, 2013, 92, S10 S11 Y. J. Mai, S. J. Shi, D. Zhang, Y. Lu, C. D. Gu, J. P. Tu, J. Power Sources, 2012, 204, M. M. Rahman, S. L. Chou, C. Zhong, J. Z. Wang, D. Wexler, H. K. Liu, Solid State Ionics, 2010, 180, S12 S. H. Choi, Y. C. Kang, ACS Appl. Mater. Interfaces, 2014, 6, S13 H. Wu, M. Xu, H. Wu, J. Xu, Y. Wang, Z. Peng, G. Zheng, J. Mater. Chem., 2012, 20, S14 Y. J. Mai, J. P. Tu, X. H. Xia, C. D. Gu, X. L. Wang, J. Power Sources, 2011, 196, S15 T. V. Thi, A. K. Rai, J. H. Gim, J. K. Kim, J. Power Sources, 2015, 292, S16 Q. Li, Y. Chen, T. Yang, D. Lei, G. Zhang, L. Mei, L. Chen, Q. Li, T. Wang, Electrochim. Acta, 2013, 90,

17 S17 X. Xu, H. Tan, K. Xi, S. Ding, D. Yu, S. Cheng, G. Yang, X. Peng, A. Fakeeh, R. V. Kumar, Carbon, 2015, 84,

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